Apparatus for treating metallic oxides



Sept. 22, 1942. B. E. CARL APPARATUS FOR TREATING METALLIC OXIDES FiledJune 29, 1940 2 Sheets-Sheet l bm i1 Sept. 22, 1942. RL

APPARATUS FOR TREATING METALLIC OXIDES Filed June 29, 1940 2sheets-sheet 2 Patented Sept. 22, 1942 OFFICE, I

. APPARATUS FOR TREATING METALLIC OXIDES Byron E. Carl, Portland, Oreg.Application June 29, 1940, Serial No. 343,079

6 Claims. (01. 266-18) My apparatus relates to the treatment of metallicoxides and its novelty consists in the adaptation and arrangement ofparts as will be more fully hereinafter pointed out.

There are tremendous deposits of low grade metallic oxides found in thenorthwest part of the United States as well as elsewhere which, becauseof the cost of recovery, have been'nonavailable.

My apparatus is adapted to eifect the complete recovery of such metallicoxides from the native ore where found at a cost which makes therecovered metals compete for the first time with the regular processesof reducing such ores from high grade deposits.

My apparatus is particularly adapted for doing this continuously andefliciently so as to reduce the cost of the operation to a point wherefor the first time the treatment of such low grade ore is practicable. I

In carrying out treatments by my apparatus I treat the metallic oxidessome of which are volatile and some of which are relatively volatilesuch as chromite, magnesium oxide, iron oxide, aluminum oxide, tungsten,titanium, manganese, vanadium, molybdenum and aluminum sulphite and rareearth metal oxides as follows:

First I grind the ore to a fine mesh between 80 and 400; second Ibeneficiate, that is concentrate the ore by removing all of theundesired material, which may be done by air blowing or by any of theother standard practices; third I calcine it to drive off all moistureand more particularly the water of combination or crystallization;fourth I mix the concentrates with at least suificient carbon to satisfythe oxygen in the ore, and this is intimately mixed for eilicientcontact with chlorine or any suitable compound of chlorine such asaluminum chloride, sulphur chloride, silicon tetra-chloride, carbontetra-chloride or hydrochloric acid; fifth I preheat this mixture to therequired temperature and maintain it at the required volatilizationtemperature of the gases formed and feed this solid preheated mixtureinto one end of a continuously revolving tube (more fully hereinafterdescribed) and the chlorine compound into the opposite end of said tubewhich is inert and impervious to the gases used and evolved in a mannerregulated so as to avoid an excess of the quantity required for thereaction and thereby contacting the solid material with said gases andvolatilizing the resulting products and fractionally condensing saidproducts. In this operation the chlorine is collected to be re-used infurther chloridizing.

' of Figure 2.

Figure 5 is a detail enlargement of the lower end of the solid feedingdevice as shown in Figure 2.

Figure 6 is a top plan view of the feeding control plate in the bottomof the solid feeding device shown in Figure 5.

In the drawings 1 is a Vitreosil (or other material inert and imperviousto the gases present) reaction tube which is mounted in a, suitableframework at each end so as to rotate at the desired speed withoutdanger of breaking or cracking and so that the material to betreated'can be continuously handled with the gases used and developedbeing imperviously contained and conducted. This framework comprises atthe feed end of said tube 1 a transit board 8, a packing 9 of asbestosgraphite and cement and bearing plates I0 are mounted thereover. Thispacking 9 is inert and impervious to the gases present in the tube 1during the entire process and also is particularly adapted to effect aperfect seal for the edge of the tube 1 at l I.

Mounted over the bearing plate [0 are the packing glands I2 and I3 whichhave a suitable packing of asbestos and graphite l4 between them andwhich are rigidly secured to the side of a hot box l5 by means of boltsl 6.

At the feed end of the tube 1 in the packing 9 is mounted a ring I1having outwardly turned fingers I8 made integral therewith and said ringI! and the fingers l8 rotating with said tube 1 and its mountings.

I9 is a rabble shaft having rabbles 20 rigidly and horizontally mountedthereon and rotating therewith, said shaft l9 being mounted in the innersolid feed tube 2| which has an outer tube 22 mounted thereover with aspace between in which is mounted a resistance wire 23 for effecting theheating of the said solid feed tube and which is connected to a sourceof current not shown.

to which is adapted to mesh with bevel gear 21 of shaft 28 supported atits outer end in a bearing 28 constituting the lower end ofbracket 38which is rigidly secured at 3| to a wall 32.

On the upper end of the feed tube 22 is rigidly secured a feed chute 34opening into the inner tube 2| so that solid feed dumped into 34 willpass into the inner tube 2 I.

Over the tube 1 is mounted a coating of asbestos cement I4 with aresistance coil I5 em- "I9 from a sourc of power not shownv continuouslycontact said contact rings I8 and II;

, Adjacent the feed end of said tube 38 is a driven gear 31 entirelysurrounding said tube 38 and rigidly mounted thereon which is engaged bythe, driving gear 38 which through crown gears 33 and 48 rotatablymounted on frame 4i are driven from the shaft 42 of an electrical motor43 of usual construction and which is adapted to be connected to asource of power (not shown) in the usual well known manner. A belt 44 isadapted to pass around the tube 38 in the channel formed by the ridges45 rigidly secured around the said tube 38 and passing over a pulley 48rigidly secured to the shaft 28 so that 'as the tube 38 is driven bymeans of the motor 43 through shaft 42 and gears 40, 38, 38 and 31 saidbelt 44 will be also driven thereby, whereby through pulley 48 shaft 28will be driven and thereby through gears 21 and 28 rabble shaft i3 willbe constantly driven at a fixed ratio of speed to that of said tube 38and the tube I contained therein. Chlorine or any suitable compound ofchlorine will be fed as described through the tube 41 from a source notshown in this drawing, thereby passing into the tube I in acontracurrent against the flow of the metallic solid matter being fedinto the feed chute 34 which passes down through the rabble I9 and whichby the rotating paddle 25 and the rotating fingers l8 will keep thesolid matter fed broken up and accessible to the solid feed end of thtube I so as to gradually feed thereinto as the tube may require.

Adjacent to the solid discharge 'end of the tube I is rigidly mounted tosolid spill box II a plate 48 having an arcuate spill slot 48 adapted tobe regulated as to its radial position by means of changing the twoscrews in the two series of screw holes 5| in order to maintain thearcuate slot 49 at. the desired height to properly regulate the level ofthe solid material in the tube I.

The discharge end of the tube I, the same as the main portion, is alsocovered by the tube 38 and a transit board 54 passes around the tube I vand an asbestos graphite cement compound packing glands u andzll arerigidly held in position i by means of bolts 88 rigidly secured to theinner end 83 of the spill box II with gas tight graphite asbestospacking 88 therebetween. Said spill box Ii has a clean out door .12 andis rigidly supported on a stand I3.

- Surrounding the lower end of the rabble feed I3 and the feed end ofthe tube I is asolid feed holder or plate II which is rigidly secured tothe inside of the hot box", which.hotbox i5 is supported on a suitablestand I8A. From the upper outer end of the hot box l5 there passes atube 82 leading into a condensation chamber 83 which has a series ofstaggered circulation plates 84 adapted to secure the varyingtemperatures required for proper condensation in said condensation box83 and the said box 83 is supported on suitable stands 85. A pipe ortube 88 is connected from the interior-of the condensation box 83 to achamber for any further separation of the gases as may be desired whichare not shown on the drawings for convenience in illustration.

Solid feed waste end of the tube 38-is supported by means of suitablestandards 81 and roller bearings 88 and the chlorine feed pipe 41 passestherethrough and tube 1 is connected directly into said spill box II asdescribed.

In carrying out the use of my apparatus the ore to be treated is firstground to a fine mesh then concentrated by removing all of the undesiredmaterial by any of the well known standard practices such as air blowingand then calcined to drive ofl all moisture and more particularly thewater of combination or crystallization. The concentrates are thenthoroughly mixed with sufficient carbon to satisfy the oxygen in the oreand this mixture is suiilciently mixed to insure efficient contact withthe chlorine or other suitable compound of chlorine as may be used. Thisthoroughly mixed compound is then preheated to the temperature requiredfor effectively carrying out the reaction sought and then fedimmediately into the feed chute 34 and as the motor 43 has already beenset in motion the shaft 42, gears 40, 33, 38, will be thereby drivenso'as to drive the driven gear 31 thereby rotating the tube 38 andthe'tube I carried therein. The belt 44 also will be driven from thebelt slot 45 through the rotation of the tube 38 whereby pulley 48 willbe driven and shaft 28, gears 21 and 28 whereby the rabble shaft i9 andthe rabbles 20 carried thereby will be rotated uniformly at desiredratio of speed with the tubes 38 and I. A regulated supply of chlorineor chlorine compound will then be allqwed to flow through the tube 41from its regulated source of supply (not shown) and the preheated solidcompoundfed down through the heated feed tube 2| will by means ofrabbles 28 gradually be fed through the openings 33 in the bottom of thefeed tube plate 24 so as to build up on the feed holder or plate 8i sothat as the rotating paddle 25 rotating with shaft l3 revolves saidsolid compound. will be gradually placed within reach of fingers I 8 ofthe ring II which constantly break up said solidcompound feed but catchsome of it gradually so as to feed it onto the open end of the revolvingtube I wherein it will be constantly rotated and tumbled further intotube I and exposed and reexposed to the action of chlorine or chlorinecompound passing through in the opposite direction in the tube I. Saidsolid compound feed will gradually build up in the tube I so as tomaintain said tube I at the desired fullness to i n-. 75 sure thecomplete exposure of all of the-,com-

- a e -12a pound feed to the action of the chlorine or other chlorinecompound so as to insure the complete .volatilizatlon of the metallicproducts sought which will pass oil with the pressure of the line of thegases into the hot box II, said gases will pass thence through tube 62into the condensation chamber 83 whereby the various desired elethepreheated solid compound will be maintained in the feed chamber 2| bymeans of the heating elements 23 and in the feed holder 6| which iscontained within the hot'box l and also the temperature in the reactiontube I will be attained and maintained by means of resistance coil I5combined with the complete insulation of said tube I.

Throughout the operation of my device the solid compound in the tube Iwill be maintained at the height desired so as to insure the completeexposure of all of the solid compound to the gases present inthe tube 1and prevent their passing through too rapidly by means of the reg.-ulation of the position of the arcuate spill slot 49 regulated by themanual adjustment of the two screws in screw holes 5 I.

It is particularly pointed out that the paddle 25 is, together with thefingers IO, a definite means for keeping the solid compound thoroughlybroken up at all times to insure its being taken into the tube I, as itrevolves, gradually and in a finely divided state so as to insure itscomplete exposure to the chlorine or other compound passing slowlythrough the rotating tube 1 whereby the solid compound is insured asteady but gradual feeding into the revolving tube I to avoid a toorapid passing through of said solid compound in said tube I and insuringin the continuou rotating and tumbling of the solid compound thecomplete exposure and reexposure to th gases present, thereby insuring acomplete reaction as to all parts of the solid compound. The action ofthe feeding mechanism for the solid compound is such that the solidcompound is always slowly approaching the edge of the rotating tube Iand the rotating tube I thereby gradually picks up the solid compoundfeeding it through the tube I only in a very gradual but continuousmanner.

It is also to be noted that my device is so contructed that therevolving tube 1 of Vitreosil or other fused silica is inert andimpervious to the gases present in the reaction described and is gastight through the gas tight packings 9 and 55 at the contacting ends ofthe tub I at II and56 and the packings l4 and 60 whereby leakage orseepage are prevented and the reaction is carried out completely andefilciently.

As surplus waste solid material is accumulated gradually in the spillbox II it can be readily removed therefrom without disturbing or interorsolid materials throughout its entire length and a solid feeding andheating mechanism at one end of said tube rotating in unison therewithand adapted'to maintain the temperature of material which has beenpreheated'at a point high enough to prevent the exiting gases passingover it from condensing and commingling therewith to avoid gumming andfeed stoppages and also keep it constantly and finely broken upandmixedand feed said solid material slowly and evenly to insurecomplete exposure and reaction, a feeding device adapted to feed aregulated counter ourtillzing chlorides above their liquifying orsolidrent of chlorine compound to said reaction tube at the opposite endof said tube a heated spill box connected with the exit-end of saidreaction tube to collect and release non-volatile chlorides, such asmagnesium chloride, and separate them from the volatile chlorides, a hotbox interposed between said reaction tube and condensation chambers tomaintain temperatures of the volaii'ying points and said fractionalcondensation chambers being attached to and interiorly conrupting thoperation of my device by opening nected with said hot box and tube sothat in said chambers the exiting volatile metallic chlorides areseparately condensed according to their liquifying or solidifying pointsand so that any one of them may be selectively removed in a relativelypure form adapted for subsequent reduction to a metal by any industrialprocesses well known to the chemical and metallurgical arts.

2. In an apparatus for recovering the metal from aluminum sulphite, arotating insulated reaction tube impervious to the gases used andevolved mounted in suitable gas tight packings having a solid feedmechanism operating in unison with said reaction tube at one end of sameand adapted to keep said solid material broken up and constantly andslowly presented to the open end of said revolving tube equipped withpick up fingers to gradually feed said solid material into said tube;adjustable means ior regulating the level of said solid feed in saidtube, vertically adjustable feeding means operating in sequence with anarcuate orifice plate positioned on the spill box at the opposite end ofsaid tube to maintain the material throughout said tube at asubstantially uniform level, means for feeding a regulated countercurrent of chlorine into said reaction tube at the end opposite saidsolid feed, means for maintaining the heat of solid material which hasbeen preheated at or above the temperature of the gases evolved, a spillbox connected with the exit end of said reaction tube to collect andrelease nonvolatile chlorides and separate them from the volatilechlorides, a hot box interposed between said reaction tube andcondensation chambers to maintain temperatures of the volatilizingchlorides above their liquifying or solidifying points and saidfractional condensation chambers attached to and internally connectedwith said hot box and tube so that in said chambers the exiting volatilemetallic chlorides are separately condensed according to theirliquiiying or solidifying points and so that any one of them may beselectively removed in a relatively pure form adapted for subsequentreduction to a metallic compound by any industrial processes well knownto the chemical and metallurgical arts.

3. In an apparatus adapted for recovering the metal from metallicoxides, a rotating heated insulated reaction tube impervious to thegases used and evolved mounted so as to rotate freely in gas tightpackings, an electric motor connecting a rabble feeding device uniformlywith said reacrotating at'a uniform speed with said reaction tube forkeeping the solid compound feed broken tion tube for solid feed whichhas been previously preheated, further adjustable means for keeping thesolid feed broken up while slowly feeding to pick up fingers ontheadjacent open end of said reaction tube, a regulated chlorine feedingdevice feeding into said reaction tube from thesation temperatures.

4. In an apparatus for recovering the metal from metallic oxides andaluminum sulphite, a rotating heated insulated reaction tube of fusedsilica having an adjustable opening at its exit end for maintaining afixed substantially uniform level of solid material throughoutits-length, a

solid feeding mechanism at the receiving end ofsaid tube rotating inunison with said reaction tube and comprising a heated rabble driven bybelt pulley shaft and gear connections from a belt slot around the outerrotating tube, a rotating paddle on the lower end of said rabble, aseries 'of cutting and breaking up fingers adjacent to the feed end ofsaid reaction tube and a feed plate, from which said solid material isthereby fed slowly and uniformly by a rotating paddle all containedwithin a hot box adjacent said feed end of said reaction tube adapted tomaintain the temperature of said preheated material and keep itconstantly and finely broken up so as to feed uniformly and slowly, afeeding device adapted to feed a regulated counter current of chlorinecompound into the exit end of said reaction tube, a solid waste spillbox connected to said exit end and a fractional condensation chamberadjoining said solid feed device.

5. In an apparatus adapted for recovering the metal from metallicoxides, a rotating heated insulated reaction tube impervious to thegases used and, evolved mounted so as to rotate'freely in gas tightpackings, a source of power connected to a series of driving gears thelast of which meshes with and drives a driven gear mounted around theinsulating tube carrying said reaction tube, a belt driven from saidinsulating tube and through a pulley shaft and gear driving a drivengear in a rabble feeding device for solid feed which has been previouslypreheated, means up while slowly and uniformly feeding to said reactiontube comprising a rotating paddle mounted on the lower end of the rabbleshaft and a ring having a series of outwardly extending fingers mountedimmediately adjacent the reaction tube and said rotating paddle, aregulated chlorine feeding device feeding into said reaction tube fromthe opposite end from said solid feed. adjustable means for maintaininga substantially. uniform height of the solid feed in said tube, a hotbox encasing said solid feed and connections, a connection from said hotbox to a condensation box of varying condensation temperatures and aconnection to a further condensing medium.

6. In an apparatus for recovering the metal evolved mounted in suitablegas tight adjustablepackings, means for maintaining a verticallyadjustable feeding mechanism operating in sequence enough to prevent theexiting gases passing over it from condensing and commingling therewithto avoid gumming and feed stoppages and adapted to maintain a uniformrotating speed or solid feed with said reaction tube and also keep saidsolid material broken up andconstantly and slowly presented to the openend of said revolving tube; means for feeding a regulated countercurrent of chlorine compound to said reaction tube at the opposite endof said tube, a spill box connected with the exit end of said reactiontube to collect and release non-volatile chlorides and separate themfrom the volatile chlorides, a hot box interposed between said reactiontube and condensation chambers to maintain temperatures of thevolatilizing chlorides above their liquifying or solidifying points andcombined with fractional condensation chambers attached to andinteriorly connected with said hot box and tube so that in said chambersthe exiting volatile metallic chlorides are separatelycondensed'according totheir liquifying or solidifying points and so thatany one of them may be selectively removed in a relatively pure formadapted for subsequent reduction to a metallic compound by anyindustrial processes well known to the chemical and metallurgical arts.

' BYRON E. CARL,

